Teknik Karakterisasi Material

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1 Teknik Karakterisasi Material
The purpose of this presentation is to give the audience a feeling about STL teaching. A. Setiabudi

2 Tujuan Perkuliahan Memberi pemahaman tentang prinsip dasar teknik karakterisasi material padat serta dasar-dasar interpretasinya Undergraduate: Basic knowledge in all areas of chemistry Intro to problem solving and analytical thinking Intro research experience Exposure to modern instrumentation and theory Exposure to interdisciplinary teams Exposure to industry via internship Become excited and stay excited about science A. Setiabudi

3 Tujuan Karakterisasi Mateial
Menentukan sifat fisika dan kimia (fisiko-kimia) Mangetahui jenis zat (atom, molekul, senyawa) Mengetahui struktur (Kristal, non kristal, ikatan) Mengetahui kemurnian Mofologi Permukaan Sifat Termal Sifat listrik A. Setiabudi

4 Characterization of Inorganic Compounds
Carry out a new chemical reaction and isolate a new/known compound (organic, inorganic, or organometallic). How do you know that your reaction has been successful or otherwise? In other words, how would you characterize the compound that you have isolated? A. Setiabudi

5 Common Questions to Ask
Does our material contains a known compound? Is it pure? What functional groups does it contain? What is its composition and its molecular weight? How the functional groups are linked to each other (connectivity)? What is the molecular symmetry? What are the bond lengths and angles? What can we say about its electronic structure? A. Setiabudi

6 Diagram Interaksi sebagai Dasar Katakteriasi Material
kalor Ion Material Foton elektron Medan Elehtromagnet neutron A. Setiabudi

7 Radiasi Elektromagnetik
Electromagnetic radiation X-ray, light, infra-red, microwave and radio waves are all e.m.r.’s, difference being their frequency thus the amount of energy they possess Spectral region of e.m.r. A. Setiabudi

8 Contoh Alur Berfikir dalam Karakterisasi
Molekuler (stuktur nya milik molekul penyusun secara individu) Teknik Spektroskopy Analisa Kimia ? Material Padat Non molekuler (atom dan ion memmbentuk struktur tiga dimensinya) XRD dan/atau analisa kimia Non Kristalin Kristalin A. Setiabudi

9 Klasifikasi Teknik Karakterisasi Material
Teknik Spektroskopy Teknik Difraksi Teknik Mikroskopy Analisa Thermal A. Setiabudi

10 Teknik Karakterisasi Material Padat
Jenis Ikatan Struktur Elektron Analisa Unsur Textur Polikristalin Struktur Permukaan Defect Kristal Struktur Kristal Unit Sel, Geometri Kristal Amorf Identifikasi Fasa XRD Difraksi Elektron dan Microscopy Difraksi Neutron Mikroscop Optik Spektroskopy IR Spektroscopy NMR, ESR Spektroscopy Elektron: XPS, UPS, AES, EELS X-Ray Spektroscopy, XRF, AEFS, EXAFS Mosebauer Spektroscopy A. Setiabudi

11 Bahan Perkuliahan Sifat Asam Basa Padatan
Spektroscopy IR untuk padatan Teknik XRF Teknik SEM dan TEM Teknik TG-DTA Teknik XRD Penentuan Luas Permukaan Padatan A. Setiabudi

12 Buku Sumber Anthony R. West, Solid state chemistry and its applications, John Willey and Sons, New York (1989) J.W. Niemansverdriet, Sepectroscopy in Catalysis, Willey-VCH, New York (2000) Sumber-sumber di internet A. Setiabudi

13 SEM A. Setiabudi

14 Pengantar: SEM Ceramic foam Perbesaran 20x A. Setiabudi

15 Pengantar: SEM Ceramic foam Perbesaran 5000x
Partikel dapat dilihat pada skala micron A. Setiabudi

16 Thermogravimetric Analysis (TGA)
thermobalance allows for monitoring sample weight as a function of temperature two most common instrument types reflection null weight calibration using calibrated weights temperature calibration based on ferromagnetic transition of Curie point standards (e.g., Ni) larger sample masses, lower temperature gradients, and higher purge rates minimize undesirable buoyancy effects For pharmaceutical samples, temperatures up to 350 °C and sample sizes of 5-20 mg are generally adequate. Reflection-type TGA (like Perkin-Elmer TGA7) depends on balance beam deflection about its fulcrum due to mass changes change in restoring force, which is proportional to the change in the sample mass, is monitored The sample hangs from the balance inside the furnace; the balance is thermally isolated from the furnace. TG curve of calcium oxalate A. Setiabudi

17 Hasil; TGA Perubahan-perubahan pada t < 850 0C serupa dg pemanasan Na3PO4 Dekomposisi Na3PO4 Reaksi Reaksi Na3PO4 dg ZrSiO4 kemungkinan terjadi pada suhu > 900 C Kurva TG-DTA pemanasan Campuran Na3PO4-ZrSiO4 A. Setiabudi

18 A modern Diffractometer
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19 Hasil XRD: Aditif Proses Pencampuran
Tujuan: menambah homogenitas campuran pra-sintering Tidak ada perbedaan signifikan antara sampel yang dipreparasi dalam bentuk serbuk dan yang diberi tekanan 60 psi A. Setiabudi